Method for preparing fluorinated polyimide film for separating arene/alkane through permeating and steaming
A polyimide membrane, polyimide technology, applied in separation methods, semi-permeable membrane separation, chemical instruments and methods, etc., can solve problems such as complex processing processes and achieve good separation effects.
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Embodiment 1
[0031] Add 110ml of DMAc (N,N-dimethylacetamide, processed by vacuum distillation before use) and 10g of diamine monomer BDAF (2,2-bis[4 -(4-aminophenoxy)phenyl]hexafluoropropane) (vacuum high-temperature dehydration before use), after the diamine monomer is completely dissolved to form a transparent solution, add 8.57g of dianhydride monomer 6FDA (4,4' -hexafluoroisopropylidene-phthalic anhydride) (purify by sublimation before use). After the reactant was completely dissolved at room temperature to form a homogeneous solution, it was moved to react in an ice-water bath for 12 hours, and then 8 g of acetic anhydride and 1.2 g of triethylamine were added with a pipette for imidization reaction for 18 hours, and the final The obtained viscous polyimide solution was poured into deionized water to precipitate out, and then taken out after repeated washing, and dried at 150° C. for 10 hours to remove the solvent to obtain the product fluorine-containing polyimide 6FDA-BDAF.
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Embodiment 2
[0045] Obtain 6FDA-BDAF material according to the operation of Example 1.
[0046] 9g of 6FDA-BDAF was dissolved in 95g of NMP, and dissolved under magnetic stirring for 24 hours to obtain a uniform and transparent polyimide solution. After the casting solution was filtered to remove impurities, vacuum defoaming was performed for 1 hour.
[0047] Cast the membrane solution on clean glass, place it under an infrared lamp to evaporate the solvent for 3 hours, take it out, and soak it in water at room temperature for 2 hours. Finally the membrane was taken out of the water and the polyimide membrane was peeled off the glass plate. The polyimide film 6FDA-BDAF thus obtained had a thickness of 17 μm.
[0048] This membrane was used to test the pervaporation separation performance of aromatics / alkanes. The feed was a toluene / n-heptane mixture with a toluene mass content of 20%. At 85°C, the permeation flux was 1.27kg·μm·m -2 h -1 , the separation factor is 4.36.
Embodiment 3
[0050] Obtain 6FDA-BDAF material according to the operation of Example 1.
[0051] 9g of 6FDA-BDAF was dissolved in 95g of DMF, and dissolved under magnetic stirring for 24 hours to finally obtain a uniform and transparent polyimide solution. After the casting solution was filtered to remove impurities, vacuum defoaming was performed for 1 hour.
[0052] Cast the membrane solution on clean glass, place it under an infrared lamp to evaporate the solvent for 2.5 hours, take it out, and soak it in water at room temperature for 2 hours. Finally the membrane was taken out of the water and the polyimide membrane was peeled off the glass plate. The polyimide film 6FDA-BDAF thus obtained had a thickness of 17 μm.
[0053] This membrane was used to test the pervaporation separation performance of aromatics / alkanes. The feed was a toluene / n-heptane mixture with a toluene mass content of 20%. At 85°C, the permeation flux was 0.64kg·μm·m -2 h -1 , the separation factor is 3.52.
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